참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Lithium Hydroxide | HCID 3939 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Methyl 2-bromo-3-methoxypropanoate | HCID 352460 | — |
| 반응물 | 3,3-Difluoropyrrolidine | HCID 2782827 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Methanol tetrahydrofuran water | HCID 21892291 | — |
| 생성물 | 2-(3,3-Difluoropyrrolidin-1-yl)-3-methoxypropanoic acid | HCID 71281227 | — |
반응 단계
A mixture of methyl 2-bromo-3-methoxypropanoate (132.0 mg, 0.66 mmol), 3,3-difluoropyrrolidine (70.6 mg, 0.66 mmol) and K2CO3 (91.2 mg, 0.66 mmol) in DMF (2 mL) was heated at 90° C. for 3 hours. The mixture was subjected to standard aqueous workup to afford a residue which was dissolved in THF/MeOH/H2O (3:2:1, 5 mL). LiOH (6N, 3.3 mmol) was added and the resulting mixture was stirred at room temperature for 30 minutes. The solution was acidified to pH5 by addition of 6N HCl. All solvents were removed under vacuum to give a crude 2-(3,3-difluoropyrrolidin-1-yl)-3-methoxypropanoic acid (58) which was used without purification. MS m/z 210.1 (M+1)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09023839B2 |
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| 출처 데이터셋 | uspto-grants-2015_05 |
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| ORD ID | ord-a5e09d88d38c468ea5828ae0f5375f94 |
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| 출처 메모 | uspto-grants-2015_05 |
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